CN1049638C - Technology for production of highly-finished sulfuric acid series product - Google Patents
Technology for production of highly-finished sulfuric acid series product Download PDFInfo
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- CN1049638C CN1049638C CN93118398A CN93118398A CN1049638C CN 1049638 C CN1049638 C CN 1049638C CN 93118398 A CN93118398 A CN 93118398A CN 93118398 A CN93118398 A CN 93118398A CN 1049638 C CN1049638 C CN 1049638C
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- sulfuric acid
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Abstract
The present invention relates to a preparation method of refined sulfuric acid and the product field of the refined sulfuric acid, which provides a novel production technology for preparing a series of refined sulfuric acid products. The novel production technology of the present invention overcomes various dilemmas and defects in the existing production technology. The present invention has the advantages of complete impurity removal, basic no pollution, little planned electric energy source consumption, stable product quality and low production cost of products. A series of products of the refined sulfuric acid can be applied to all fields using the refined sulfuric acid.
Description
The present invention relates to, industrial goods sulfuric acid is carried out refinement treatment, and obtain the technical field of highly-finished sulfuric acid series product.
Highly-finished sulfuric acid series product can be categorized as by its end-use: reagent of sulfuric acid, foodstuff additive sulfuric acid, industrial POV three major types.
At present, the existing production technology of reagent of sulfuric acid has: distillation method and distillation method after chemical treatment.Its main drawback is that current consumption is big, the production cost height.
At present, the existing production technology of industrial POV; (1) uses the industry law of the reforming gas of contact process as raw material; (2) after chemical treatment is refining, concentrate or the redistillation method, use the industry law of the reforming gas of contact process as raw material for (1), the product of domestic production producer, how because of the expensive letter system of the investment of equipment and tubing, its quality product is defective.Concentrate or the redistillation method after chemical treatment is refining for (2), its chemical treating process has again; (1) common hydrogen sulfide method, (2) first nitric acid oxidation is used precipitation agent again, and for example: yellow prussiate of potash, materials such as Sodium phosphate dibasic carry out removal of impurities and handle, (3) other workshop-based processing simple or mutation.The main drawback of these treating processess is that removal of impurities can not be complete, nitric acid smog severe contamination, and quality product is difficult to meet the countries concerned's standard (product is defective).Full technological process is discontinuous mutually, present treat the head when the head aches, pin cures the pin phenomenon bitterly, the production cost height must make professional production producer be difficult to survive in for many years.Therefore, for many years, have more existing replacement or substitute on the market, for example, substitute store battery sulfuric acid with solid sulphuric acid or colloid sulfuric acid.As if substitute plating dosing POV with defective reagent of sulfuric acid, this existing production technology that also means industrial POV " has been gone to the end ".
Purpose of the present invention in order to overcome the various shortcomings that above-mentioned existing production technology exists, provides a kind of new process of production of producing highly-finished sulfuric acid series product just, is applicable to the purposes field of whole POV to realize its series product.
The present invention has used three ultimate principles in chemical field and the chemical field, thereby forms the new process of production process of " system's removal of impurities " naturally, can be described as " displacement impurity removed system technology ".
The product of the present invention's trial-production is in December, 1991 and in June, 1992, through test of this province Zunyi State Bureau of Technical Supervision and approval.
Below, clear description the present invention produces the new process of production of highly-finished sulfuric acid series product.Mainly contain: complex acid, displacement, heating, concentrated or four steps of fractionation, existing division is as follows:
One, complex acid
Industrial goods sulfuric acid is made into the solution of 10-50% (weight percent) with pure water (distilled water, or deionized water).The complex acid method can only under continuous agitation condition, add the industrial goods vitriol oil in the pure water lentamente.
Two, displacement reaction
Displacer is in the chemical knowledge field, the metal in the metal activity command table before the iron (Fe).Preferably highly purified aluminium or zinc.
By 1 part of weight of industrial goods sulfuric acid (proportion is 1.83-1.84), take by weighing above-mentioned displacer 0.02-0.08 part weight, displacer and " one, complex acid " gained solution are carried out replacement(metathesis)reaction.Control reacting liquid temperature at 20-60 ℃, in the reaction process, every 15-30 minute, stirring reaction liquid 1-2 minute.Visual inspection (or from task equipment of the present invention " displacing device " equipment manhole observe) sees that solution presents that tiny bubble is vaporific is advisable.Treat that replacement(metathesis)reaction carried out 1-4 hour, solution is carried out normal pressure filter.Filter residue effluxes.Filtrate is used for heating.
Displacement main reaction formula: (make that displacer is A, its ion is A
a)
This replacement(metathesis)reaction is preferably in the task equipment of the present invention " displacing device " and carries out, so that control conditions of replacement reaction and series operation.Replacement(metathesis)reaction is emitted the pungent gas with foreign flavor of sulfur-bearing acid mist simultaneously, after environmental protection treatment, obtains purified hydrogen product.
Because the employing of replacement(metathesis)reaction; make a large amount of displacer ions enter solution, so, how the displacer ion is discharged solution? in the existing production technology; which uses some precipitation agent to make the displacer ion become the precipitation elimination methods, has all run into " crisis " to some extent at this.But, by the present invention, use following heating and spissated method, can easyly integratedly technological process be gone on smoothly naturally again, and the quality of series product is guaranteed, receive beyond thought effect.
Three, heating
In the filtrate solution of " two, replacement(metathesis)reaction " gained, by the weight of raw material acid per ton (proportion is 1.83-1.84), add 1: 1 nitric acid 30-50 milliliter, add after 1: 1 hydrogen peroxide 20-30 milliliter, solution is carried out heating evaporation.The heat supply of heated solution can adopt the combustion heat energy of fire coal (or other cheap fuel) to realize, and without the electric power energy heat supply.
When treating that strength of solution reaches 50-60% (weight percent), stop heating.The careful hydrothermal solution that stirs, make present muddy slag after, restir 1-3 minute.Treat that solution is chilled to room temperature and carries out the normal pressure filtration, filter residue reclaims dries, and promptly gets the product of paying of economic worth, perhaps filter residue is handled purification, and filtrate is for concentrating or the fractionation use.
Four, concentrated or fractionation
1. concentrate
" three, heating " gained filtrate is concentrated.Collect vapour and cigarette that concentrated solution is emitted, gained phlegma sulfur acid is below 2%.Treat that strength of solution reaches at 92% o'clock, stops heat supply.Careful stir the existing slag of hydrothermal solution after, restir 1-3 minute, treat that solution cools to (120 ± 20) ℃, carries out normal pressure with solution and filters.Filter residue reclaims, and promptly gets the product of paying of economic worth.Concentrate heat supply and " three, heating " with.
Filtrate is through leaving standstill cooling more than 24 hours, again through negative pressure leaching, that gained filtrate is is industrial (or foodstuff additive with) highly-finished sulfuric acid series product.
2, fractionation
" three, heating " gained filtrate is carried out fractionation.The heat supply of the electrification energy.
Fractionation operation belongs to prior art, carries out fractionation operation by standard equipment specification and the key points for operation selected.It collects liquid, is reagent Sulfuric Acid Series product.
Fractionated vapour condensation liquid also need be collected to reclaim and use.
Use advantage of the present invention:
1. use removal of impurities of the present invention can be complete, guarantees that series product of the present invention reach its countries concerned's standard.For example: reagent meets or exceeds GB625-89 with priority pure product, and industrial POV product (store battery with the agricultural sour product of sulfuric acid one-level) meet or exceed GB4554-84.
2. the series product produced of the present invention are applicable to whole purposes field of POV.
3. enforcement the present invention realizes pollution-free substantially.
4. use the product of the present invention's production, its steady quality.
5. use the present invention reduces the application plan electric power energy in a large number.
6. use the products production cost of the present invention's production, the products production cost of producing than prior art reduces relatively.
7. enforcement the present invention, outside the investigation of replacement(metathesis)reaction, the hydrogen that all the other obtained, phlegma and precipitation all are the products of paying that can utilize economic worth, therefore, implement ratio defective product of the present invention, up to more than 99.9%.Implement the POV ratio defective product that the present invention produces, up to more than 97%.
Embodiment
Undertaken by aforementioned processing method is described.Wherein: complex acid concentration is 20-30%, and the replacement(metathesis)reaction temperature is 30-40 ℃, and its reaction times is 1-3 hour, and amount ratio is: raw material acid: high-purity Zn=1: 0.02-0.05 (weight ratio).Through concentrating gained POV product, be industrial (or foodstuff additive are used).Use for agent on probation through fractionation gained POV product.(table is seen the literary composition back)
The quality index project name quality index of POV product
The reagent industrial one-level concentrated acid of top grade straight product sulfur acid (H
2SO
4), % 95-98＞92 residues, %＜0.0005＜0.03 chlorine (Cl), %＜0.00001＜0.00002 iron (Fe), %＜0.00001＜0.0001 ammonium (NH
4 +), the no nitrogen of % (N), %＜0.00001＜0.00001 arsenic (As), %＜0.000001＜0.00001 heavy metal, %＜0.00001＜0.0001 reduction potassium permanganate material, %＜0.0001＜0.001 manganese＜Mn) %-＜0.00002 outward appearance is qualified
Claims (1)
1. the new process of production of a POV product, it is characterized in that, adopt industrial goods sulfuric acid and the displacer metal of compound concentration at 10-50%, be raffinal or zinc, carry out replacement(metathesis)reaction, control reaction temperature is at 20-60 ℃, every 15 ℃ of-30 minutes stirring reaction liquid 1-2 minute, reacts 1-4 hour, solution is carried out normal pressure to be filtered, when again its gained filtrate heating being reached weight percent concentration 50-60%, stop heating, restir was 1-3 minute after stirring was slagged tap, be chilled to room temperature and carry out the normal pressure filtration, again its gained filtrate is concentrated or the branch gold-plating, stop heat supply when concentrated solution concentration reaches 92%, restir was 1-3 minute after stirring was slagged tap, and make cooling solution be carried out the normal pressure filtration at 100-140 ℃, filtrate is left standstill and is cooled off more than 24 hours, again through negative pressure leaching, divides the gold-plating operation to be undertaken by original technical requirements.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN93118398A CN1049638C (en) | 1993-10-01 | 1993-10-01 | Technology for production of highly-finished sulfuric acid series product |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN93118398A CN1049638C (en) | 1993-10-01 | 1993-10-01 | Technology for production of highly-finished sulfuric acid series product |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1101008A CN1101008A (en) | 1995-04-05 |
| CN1049638C true CN1049638C (en) | 2000-02-23 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN93118398A Expired - Fee Related CN1049638C (en) | 1993-10-01 | 1993-10-01 | Technology for production of highly-finished sulfuric acid series product |
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| Country | Link |
|---|---|
| CN (1) | CN1049638C (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100441500C (en) * | 2004-04-19 | 2008-12-10 | 上海京藤化工有限公司 | Production method of refined sulfuric acid and production equipment thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5026535A (en) * | 1988-11-16 | 1991-06-25 | Boliden Contech Ab | Method for decoloring sulphuric acid deriving from acid production processes |
-
1993
- 1993-10-01 CN CN93118398A patent/CN1049638C/en not_active Expired - Fee Related
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5026535A (en) * | 1988-11-16 | 1991-06-25 | Boliden Contech Ab | Method for decoloring sulphuric acid deriving from acid production processes |
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| Publication number | Publication date |
|---|---|
| CN1101008A (en) | 1995-04-05 |
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